Limonene extraction of cannabis

[HashoftheTitans]

Does water and limonene form an azeotrope? Arent they immiscible? I dont think the lower BP of a mixture means azeotrope, especially if they are immiscible.

I don't have a background in chemistry but I have jumped into the world of Limonene extraction. I can tell you that Limonene distills like a dream in the presence of the right amount of water and vacuum. I had it cold distilling at 47F at one point. I was rocking 130 rpm in a 20 L rotovap and pushing bumping limits to the max. Those temps are highly inefficient and I found that Limonene poured down my condenders at almost a 5/1 ratio when distilled at 120F.

 

[Pangea]

Cool! How are you finding the process and end results? When you say you almost get a 5/1 ratio of distillate, what ratio do you start with in your distillation flask?

 

[HashoftheTitans]

I start at 50/50 and add Limonene as boils down. I add water if it wants to bump. Things Getty violent if there is not enough water present. I distilled 5 gallons and got a significant amount of foul orange-smelling "mystery oil"

 

[Pangea]

What is the purity of the limonene you start with before purifying? Are you collecting/discarding any fractions of the condensate?

Are you doing similar boil downs when purging extracts?

 

[HashoftheTitans]

99.4%. Condensate is just Limonene and water as far as I can tell. I only did a trial run so I haven't refined my technique.

 

[Pangea]

Thanks for sharing, cool to hear more folks are testing it out.

I ask about condensate fractions because boiling and condensing an impure liquid mixture will not result in a pure condensate especially if the boiling points are similar and not well fractionated. Imagine if the impurities where terpenes, after running/extracting a few pounds of herb with a few gallons of the same limonene it should be contaminated with low levels of other terpenes, especially the likes of linalool which has a close density and bp as limonene.

I wonder about how the starting limonene was purified to 99.4% and why there is more than .6% by weight on average left over mystery oil? If the common limonene or high purity limonene on the market is made and purified in the same manner as what limonene extractors are doing, which is steam distillation, then why isnt there a higher purity or mystery oil free grade of oil available commercially?

I wonder if any limonene folks have tested their mystery oil? Or their limonene after larger batches of extraction.

 

[HashoftheTitans]

I saw a patented purification process where they used an oxidizer and then acidified, then followed by water washes and separated.

 

[hash head]

I boiled mine off at about 120f. The bulk of it came out pretty quickly. I used about a gallon of water to distill a pint in less than an hour.

Did you use a 5l rotovap?

 

[hash head]

Does water and limonene form an azeotrope? Arent they immiscible? I dont think the lower BP of a mixture means azeotrope, especially if they are immiscible.

yes they form an azeotrope and it lowers the boiling point to below that of water.

 

[Pangea]

I completely agree that the mixture creates a lower boiling point, but to be pedantic, as far as I am aware they are not forming a azeotrope as they are not miscible. A mixture of one or more components does not need be a azeotrope to create a lower BP.

 

[Lyfespan]

this extraction method is why we have all these tangie,lemon tree sap waxes around huh

 

[regseeds]

RIP Horatio Delbert
Saved so many lives, fell pretty sick right now.

Legend - What a guy

https://www.gofundme.com/f/horatio-delbert

 

[Benny106]

Shit man. Rip, I loved hearing his take on things via hash church.

 

[Lyfespan]

did someone hit him in the head, or did he fall, does anyone know what really happened to Horatio

 

[whereisbrianV.]

A triclamp failure while the vessel and cap were under pressure. Apparently it was a Co2/d-lime cxe type of extraction so the pressures where likely above 100bar. It's a very sad reminder of the dangers of Co2 extraction, not at all as benign as it's marketed as being.